Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email patrickm@chem.leeds.ac.uk _publ_contact_author_name 'Patrick C. McGowan' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Patrick C. McGowan Department of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 343 6404' _publ_contact_author_fax '+44 (0)113 343 6565' #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Mono-Amino-Functionalised Ferrocene, Ferrocene Salts, Ferrocenium Salts ; loop_ _publ_author_name _publ_author_address 'Stephen J. Furtado' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Andrew L. Gott' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Patrick C. McGowan' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; #=====END data_sjf129-4 _database_code_depnum_ccdc_archive 'CCDC 219613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 F3 Fe N O2' _chemical_formula_weight 397.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7312(1) _cell_length_b 10.6343(2) _cell_length_c 10.8930(2) _cell_angle_alpha 76.8424(8) _cell_angle_beta 70.3960(6) _cell_angle_gamma 68.5129(8) _cell_volume 880.17(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8409 _exptl_absorpt_correction_T_max 0.8409 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18894 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4036 _reflns_number_gt 3734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.3111P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.028(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4036 _refine_ls_number_parameters 255 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.24050(3) 0.75309(2) 0.92285(2) 0.02398(10) Uani 1 1 d . . . F1 F 0.5632(11) 0.6698(9) 0.1884(6) 0.082(2) Uani 0.50 1 d PD A 1 F2 F 0.5971(6) 0.6291(5) 0.3793(7) 0.0818(15) Uani 0.50 1 d PD A 1 F3 F 0.5211(4) 0.8317(4) 0.3024(7) 0.0856(15) Uani 0.50 1 d PD A 1 F11 F 0.5775(10) 0.6461(6) 0.2037(8) 0.076(2) Uani 0.50 1 d PD A 2 F12 F 0.5889(8) 0.7132(11) 0.3596(5) 0.135(3) Uani 0.50 1 d PD A 2 F13 F 0.4763(5) 0.8524(3) 0.2148(4) 0.0762(11) Uani 0.50 1 d PD A 2 O1 O 0.28121(18) 0.61668(14) 0.35771(14) 0.0431(3) Uani 1 1 d . . . O2 O 0.21801(17) 0.81292(13) 0.43549(14) 0.0422(3) Uani 1 1 d . . . N14 N -0.07964(18) 0.76269(14) 0.55875(13) 0.0286(3) Uani 1 1 d . . . H14 H 0.0209 0.7843 0.5157 0.034 Uiso 1 1 calc R . . C1 C 0.4975(2) 0.69869(19) 0.89611(18) 0.0345(4) Uani 1 1 d . . . H1 H 0.5593 0.6334 0.9524 0.041 Uiso 1 1 calc R . . C2 C 0.4199(2) 0.84045(18) 0.90726(17) 0.0330(4) Uani 1 1 d . . . H2 H 0.4215 0.8863 0.9720 0.040 Uiso 1 1 calc R . . C3 C 0.3399(2) 0.90143(17) 0.80481(17) 0.0313(4) Uani 1 1 d . . . H3 H 0.2783 0.9951 0.7891 0.038 Uiso 1 1 calc R . . C4 C 0.3682(2) 0.79723(18) 0.72972(16) 0.0320(4) Uani 1 1 d . . . H4 H 0.3285 0.8093 0.6553 0.038 Uiso 1 1 calc R . . C5 C 0.4663(2) 0.67189(18) 0.78603(18) 0.0336(4) Uani 1 1 d . . . H5 H 0.5043 0.5857 0.7555 0.040 Uiso 1 1 calc R . . C6 C 0.1230(2) 0.60626(16) 0.99412(16) 0.0274(3) Uani 1 1 d . . . H6 H 0.1660 0.5173 0.9687 0.033 Uiso 1 1 calc R . . C7 C 0.1557(2) 0.64515(18) 1.09757(16) 0.0312(4) Uani 1 1 d . . . H7 H 0.2237 0.5868 1.1530 0.037 Uiso 1 1 calc R . . C8 C 0.0686(2) 0.78654(18) 1.10296(16) 0.0313(4) Uani 1 1 d . . . H8 H 0.0684 0.8394 1.1626 0.038 Uiso 1 1 calc R . . C9 C -0.0184(2) 0.83537(17) 1.00318(16) 0.0275(3) Uani 1 1 d . . . H9 H -0.0868 0.9265 0.9852 0.033 Uiso 1 1 calc R . . C10 C 0.0144(2) 0.72435(16) 0.93487(15) 0.0253(3) Uani 1 1 d . . . C11 C -0.0629(2) 0.72720(15) 0.82962(15) 0.0248(3) Uani 1 1 d . . . H11 H -0.1713 0.7042 0.8744 0.030 Uiso 1 1 calc R . . C12 C 0.0517(2) 0.62143(16) 0.73505(15) 0.0272(3) Uani 1 1 d . . . H12A H 0.1617 0.6400 0.6904 0.033 Uiso 1 1 calc R . . H12B H 0.0769 0.5298 0.7854 0.033 Uiso 1 1 calc R . . C13 C -0.0324(2) 0.62340(16) 0.63280(16) 0.0303(3) Uani 1 1 d . . . H13A H 0.0474 0.5571 0.5708 0.036 Uiso 1 1 calc R . . H13B H -0.1367 0.5960 0.6765 0.036 Uiso 1 1 calc R . . C14 C -0.1598(3) 0.7640(2) 0.45763(19) 0.0415(4) Uani 1 1 d . . . H14A H -0.2627 0.7363 0.5001 0.062 Uiso 1 1 calc R . . H14B H -0.0783 0.7006 0.3949 0.062 Uiso 1 1 calc R . . H14C H -0.1914 0.8561 0.4112 0.062 Uiso 1 1 calc R . . C15 C -0.1939(2) 0.86817(17) 0.64874(16) 0.0294(3) Uani 1 1 d . . . H15A H -0.3041 0.8498 0.6932 0.035 Uiso 1 1 calc R . . H15B H -0.2184 0.9591 0.5969 0.035 Uiso 1 1 calc R . . C16 C -0.1108(2) 0.86792(16) 0.75076(16) 0.0283(3) Uani 1 1 d . . . H16A H -0.1909 0.9356 0.8113 0.034 Uiso 1 1 calc R . . H16B H -0.0064 0.8950 0.7066 0.034 Uiso 1 1 calc R . . C17 C 0.3119(2) 0.71572(17) 0.37040(17) 0.0315(4) Uani 1 1 d . A . C18 C 0.4936(3) 0.7235(2) 0.2977(2) 0.0495(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02172(15) 0.02496(15) 0.02496(15) -0.00176(9) -0.00530(9) -0.00886(10) F1 0.063(4) 0.158(7) 0.0333(18) -0.027(3) 0.006(2) -0.052(4) F2 0.0332(18) 0.092(3) 0.122(4) -0.018(3) -0.035(2) -0.0066(19) F3 0.0350(18) 0.0428(18) 0.166(5) -0.031(2) 0.008(2) -0.0194(14) F11 0.043(3) 0.0511(19) 0.112(5) -0.044(2) 0.024(3) -0.0109(16) F12 0.075(4) 0.308(11) 0.074(3) -0.051(6) -0.017(3) -0.107(7) F13 0.0453(18) 0.0515(18) 0.100(3) 0.0089(18) 0.0109(18) -0.0184(14) O1 0.0436(8) 0.0427(7) 0.0480(8) -0.0156(6) -0.0085(6) -0.0171(6) O2 0.0389(7) 0.0324(7) 0.0485(8) -0.0109(6) 0.0048(6) -0.0153(6) N14 0.0299(7) 0.0313(7) 0.0262(7) -0.0002(5) -0.0077(6) -0.0134(6) C1 0.0225(8) 0.0378(9) 0.0411(9) -0.0007(7) -0.0085(7) -0.0100(7) C2 0.0280(8) 0.0396(9) 0.0357(9) -0.0073(7) -0.0046(7) -0.0177(7) C3 0.0281(8) 0.0290(8) 0.0334(8) -0.0006(7) -0.0022(7) -0.0128(7) C4 0.0282(8) 0.0401(9) 0.0282(8) -0.0042(7) -0.0020(7) -0.0165(7) C5 0.0244(8) 0.0329(8) 0.0398(9) -0.0094(7) 0.0001(7) -0.0102(7) C6 0.0270(8) 0.0258(7) 0.0293(8) 0.0022(6) -0.0079(6) -0.0115(6) C7 0.0302(8) 0.0359(9) 0.0283(8) 0.0047(7) -0.0098(7) -0.0147(7) C8 0.0310(9) 0.0387(9) 0.0247(7) -0.0043(7) -0.0043(6) -0.0144(7) C9 0.0233(7) 0.0301(8) 0.0271(8) -0.0040(6) -0.0036(6) -0.0087(6) C10 0.0224(7) 0.0276(7) 0.0250(7) -0.0010(6) -0.0040(6) -0.0106(6) C11 0.0226(7) 0.0249(7) 0.0262(7) -0.0011(6) -0.0056(6) -0.0091(6) C12 0.0291(8) 0.0238(7) 0.0291(8) -0.0015(6) -0.0083(6) -0.0096(6) C13 0.0361(9) 0.0272(8) 0.0310(8) -0.0015(6) -0.0096(7) -0.0150(7) C14 0.0486(11) 0.0500(11) 0.0328(9) -0.0013(8) -0.0184(8) -0.0192(9) C15 0.0276(8) 0.0287(8) 0.0301(8) -0.0005(6) -0.0088(7) -0.0078(6) C16 0.0289(8) 0.0244(7) 0.0312(8) -0.0018(6) -0.0099(7) -0.0075(6) C17 0.0307(8) 0.0315(8) 0.0317(8) -0.0030(7) -0.0101(7) -0.0084(7) C18 0.0328(10) 0.0512(12) 0.0656(14) -0.0247(10) -0.0029(9) -0.0137(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.0351(17) . ? Fe1 C2 2.0401(17) . ? Fe1 C7 2.0421(16) . ? Fe1 C8 2.0442(17) . ? Fe1 C6 2.0443(16) . ? Fe1 C9 2.0529(16) . ? Fe1 C5 2.0546(17) . ? Fe1 C3 2.0554(16) . ? Fe1 C4 2.0612(17) . ? Fe1 C10 2.0638(15) . ? F1 C18 1.297(6) . ? F2 C18 1.443(6) . ? F3 C18 1.274(4) . ? F11 C18 1.304(6) . ? F12 C18 1.198(5) . ? F13 C18 1.447(4) . ? O1 C17 1.224(2) . ? O2 C17 1.251(2) . ? N14 C14 1.486(2) . ? N14 C15 1.496(2) . ? N14 C13 1.499(2) . ? C1 C5 1.423(3) . ? C1 C2 1.423(3) . ? C2 C3 1.420(2) . ? C3 C4 1.426(2) . ? C4 C5 1.425(3) . ? C6 C7 1.427(2) . ? C6 C10 1.436(2) . ? C7 C8 1.420(2) . ? C8 C9 1.427(2) . ? C9 C10 1.428(2) . ? C10 C11 1.503(2) . ? C11 C12 1.529(2) . ? C11 C16 1.533(2) . ? C12 C13 1.519(2) . ? C15 C16 1.516(2) . ? C17 C18 1.541(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 40.89(7) . . ? C1 Fe1 C7 104.02(7) . . ? C2 Fe1 C7 118.22(7) . . ? C1 Fe1 C8 121.80(7) . . ? C2 Fe1 C8 105.89(7) . . ? C7 Fe1 C8 40.66(7) . . ? C1 Fe1 C6 118.80(7) . . ? C2 Fe1 C6 153.82(7) . . ? C7 Fe1 C6 40.88(7) . . ? C8 Fe1 C6 68.51(7) . . ? C1 Fe1 C9 160.13(7) . . ? C2 Fe1 C9 125.04(7) . . ? C7 Fe1 C9 68.49(7) . . ? C8 Fe1 C9 40.77(6) . . ? C6 Fe1 C9 68.33(6) . . ? C1 Fe1 C5 40.71(7) . . ? C2 Fe1 C5 68.47(7) . . ? C7 Fe1 C5 122.51(7) . . ? C8 Fe1 C5 158.83(8) . . ? C6 Fe1 C5 107.04(7) . . ? C9 Fe1 C5 158.71(7) . . ? C1 Fe1 C3 68.50(7) . . ? C2 Fe1 C3 40.58(7) . . ? C7 Fe1 C3 154.85(7) . . ? C8 Fe1 C3 121.55(7) . . ? C6 Fe1 C3 163.82(7) . . ? C9 Fe1 C3 110.04(7) . . ? C5 Fe1 C3 68.28(7) . . ? C1 Fe1 C4 68.39(7) . . ? C2 Fe1 C4 68.29(7) . . ? C7 Fe1 C4 160.85(7) . . ? C8 Fe1 C4 158.25(7) . . ? C6 Fe1 C4 126.02(7) . . ? C9 Fe1 C4 124.29(7) . . ? C5 Fe1 C4 40.52(7) . . ? C3 Fe1 C4 40.54(7) . . ? C1 Fe1 C10 155.77(7) . . ? C2 Fe1 C10 162.97(7) . . ? C7 Fe1 C10 68.94(6) . . ? C8 Fe1 C10 68.74(6) . . ? C6 Fe1 C10 40.93(6) . . ? C9 Fe1 C10 40.59(6) . . ? C5 Fe1 C10 122.35(7) . . ? C3 Fe1 C10 127.37(7) . . ? C4 Fe1 C10 110.37(7) . . ? C14 N14 C15 111.04(14) . . ? C14 N14 C13 110.61(13) . . ? C15 N14 C13 111.73(12) . . ? C5 C1 C2 108.08(16) . . ? C5 C1 Fe1 70.38(10) . . ? C2 C1 Fe1 69.74(10) . . ? C3 C2 C1 108.12(15) . . ? C3 C2 Fe1 70.29(9) . . ? C1 C2 Fe1 69.37(9) . . ? C2 C3 C4 107.94(15) . . ? C2 C3 Fe1 69.13(9) . . ? C4 C3 Fe1 69.95(9) . . ? C5 C4 C3 107.98(15) . . ? C5 C4 Fe1 69.49(10) . . ? C3 C4 Fe1 69.51(9) . . ? C1 C5 C4 107.87(15) . . ? C1 C5 Fe1 68.91(10) . . ? C4 C5 Fe1 69.99(10) . . ? C7 C6 C10 108.50(14) . . ? C7 C6 Fe1 69.48(9) . . ? C10 C6 Fe1 70.27(9) . . ? C8 C7 C6 107.88(14) . . ? C8 C7 Fe1 69.75(9) . . ? C6 C7 Fe1 69.64(9) . . ? C7 C8 C9 108.09(14) . . ? C7 C8 Fe1 69.59(9) . . ? C9 C8 Fe1 69.94(9) . . ? C8 C9 C10 108.63(14) . . ? C8 C9 Fe1 69.29(9) . . ? C10 C9 Fe1 70.12(9) . . ? C9 C10 C6 106.90(14) . . ? C9 C10 C11 126.63(14) . . ? C6 C10 C11 126.25(14) . . ? C9 C10 Fe1 69.29(9) . . ? C6 C10 Fe1 68.81(9) . . ? C11 C10 Fe1 131.03(11) . . ? C10 C11 C12 112.95(13) . . ? C10 C11 C16 112.93(13) . . ? C12 C11 C16 109.20(13) . . ? C13 C12 C11 111.72(13) . . ? N14 C13 C12 110.68(13) . . ? N14 C15 C16 110.95(13) . . ? C15 C16 C11 111.47(13) . . ? O1 C17 O2 129.79(17) . . ? O1 C17 C18 116.38(16) . . ? O2 C17 C18 113.82(16) . . ? F12 C18 F3 63.0(5) . . ? F12 C18 F1 116.2(5) . . ? F3 C18 F1 117.8(5) . . ? F12 C18 F11 108.3(6) . . ? F3 C18 F11 124.3(5) . . ? F1 C18 F11 12.4(7) . . ? F12 C18 F2 36.2(5) . . ? F3 C18 F2 99.2(4) . . ? F1 C18 F2 101.4(5) . . ? F11 C18 F2 89.6(5) . . ? F12 C18 F13 107.3(5) . . ? F3 C18 F13 47.0(3) . . ? F1 C18 F13 85.1(4) . . ? F11 C18 F13 96.7(4) . . ? F2 C18 F13 141.8(3) . . ? F12 C18 C17 119.5(3) . . ? F3 C18 C17 116.3(2) . . ? F1 C18 C17 114.6(4) . . ? F11 C18 C17 114.6(4) . . ? F2 C18 C17 103.6(3) . . ? F13 C18 C17 107.7(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.596 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.097 #===END data_sjf129-5 _database_code_depnum_ccdc_archive 'CCDC 219614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 B F4 Fe N' _chemical_formula_weight 371.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2374(1) _cell_length_b 7.8466(1) _cell_length_c 20.5146(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.7630(5) _cell_angle_gamma 90.00 _cell_volume 1647.74(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8325 _exptl_absorpt_correction_T_max 0.8325 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44011 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3784 _reflns_number_gt 3351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.5961P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3784 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.51042(2) 0.90619(3) 0.243628(10) 0.02654(10) Uani 1 1 d . . . F1 F 0.31997(13) 0.42132(14) -0.04562(7) 0.0560(3) Uani 1 1 d . . . F2 F 0.34284(13) 0.23087(18) 0.03662(7) 0.0613(3) Uani 1 1 d . . . F3 F 0.15518(11) 0.38557(13) 0.02475(6) 0.0420(3) Uani 1 1 d . . . F4 F 0.20429(12) 0.17560(15) -0.04728(6) 0.0497(3) Uani 1 1 d . . . N14 N 0.20650(13) 0.73855(17) -0.00201(6) 0.0281(3) Uiso 1 1 d . . . H14 H 0.2060 0.6217 0.0055 0.034 Uiso 1 1 calc R . . C1 C 0.57469(18) 1.0901(2) 0.18187(9) 0.0364(4) Uani 1 1 d . . . H1 H 0.5389 1.1147 0.1400 0.044 Uiso 1 1 calc R . . C2 C 0.67689(17) 0.9716(2) 0.19566(9) 0.0373(4) Uani 1 1 d . . . H2 H 0.7214 0.9038 0.1647 0.045 Uiso 1 1 calc R . . C3 C 0.70034(16) 0.9732(2) 0.26430(9) 0.0370(4) Uani 1 1 d . . . H3 H 0.7633 0.9064 0.2872 0.044 Uiso 1 1 calc R . . C4 C 0.61326(18) 1.0918(2) 0.29251(9) 0.0370(4) Uani 1 1 d . . . H4 H 0.6075 1.1179 0.3376 0.044 Uiso 1 1 calc R . . C5 C 0.53557(18) 1.1652(2) 0.24142(9) 0.0370(4) Uani 1 1 d . . . H5 H 0.4696 1.2492 0.2464 0.044 Uiso 1 1 calc R . . C6 C 0.46074(16) 0.6687(2) 0.21106(8) 0.0300(3) Uani 1 1 d . . . H6 H 0.5087 0.6006 0.1815 0.036 Uiso 1 1 calc R . . C7 C 0.47549(16) 0.6680(2) 0.28059(8) 0.0325(3) Uani 1 1 d . . . H7 H 0.5352 0.6000 0.3051 0.039 Uiso 1 1 calc R . . C8 C 0.38527(16) 0.7865(2) 0.30640(8) 0.0339(4) Uani 1 1 d . . . H8 H 0.3737 0.8111 0.3513 0.041 Uiso 1 1 calc R . . C9 C 0.31480(15) 0.8626(2) 0.25337(8) 0.0301(3) Uani 1 1 d . . . H9 H 0.2486 0.9469 0.2569 0.036 Uiso 1 1 calc R . . C10 C 0.36134(14) 0.7897(2) 0.19373(7) 0.0270(3) Uani 1 1 d . . . C11 C 0.31207(14) 0.8347(2) 0.12651(7) 0.0266(3) Uani 1 1 d . . . H11 H 0.3148 0.9615 0.1219 0.032 Uiso 1 1 calc R . . C12 C 0.39686(15) 0.7572(2) 0.07327(7) 0.0312(3) Uani 1 1 d . . . H12A H 0.4871 0.8013 0.0780 0.037 Uiso 1 1 calc R . . H12B H 0.3999 0.6320 0.0789 0.037 Uiso 1 1 calc R . . C13 C 0.34534(15) 0.7984(2) 0.00524(7) 0.0307(3) Uani 1 1 d . . . H13A H 0.3496 0.9229 -0.0023 0.037 Uiso 1 1 calc R . . H13B H 0.4002 0.7415 -0.0276 0.037 Uiso 1 1 calc R . . C14 C 0.15447(18) 0.7668(2) -0.06947(8) 0.0370(4) Uani 1 1 d . . . H14A H 0.1541 0.8892 -0.0791 0.055 Uiso 1 1 calc R . . H14B H 0.0652 0.7224 -0.0728 0.055 Uiso 1 1 calc R . . H14C H 0.2100 0.7075 -0.1007 0.055 Uiso 1 1 calc R . . C15 C 0.12102(15) 0.8191(2) 0.04793(8) 0.0326(3) Uani 1 1 d . . . H15A H 0.0303 0.7773 0.0422 0.039 Uiso 1 1 calc R . . H15B H 0.1206 0.9443 0.0419 0.039 Uiso 1 1 calc R . . C16 C 0.17027(15) 0.7763(2) 0.11622(7) 0.0310(3) Uani 1 1 d . . . H16A H 0.1646 0.6517 0.1232 0.037 Uiso 1 1 calc R . . H16B H 0.1140 0.8327 0.1486 0.037 Uiso 1 1 calc R . . B1 B 0.25749(19) 0.3012(3) -0.00757(10) 0.0348(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02430(14) 0.03147(16) 0.02383(14) -0.00030(8) -0.00045(9) -0.00143(8) F1 0.0549(7) 0.0359(6) 0.0780(9) 0.0050(5) 0.0327(7) 0.0019(5) F2 0.0553(7) 0.0604(8) 0.0676(8) 0.0049(6) -0.0171(6) 0.0094(6) F3 0.0411(6) 0.0372(6) 0.0481(6) -0.0035(4) 0.0147(5) -0.0005(4) F4 0.0527(7) 0.0401(6) 0.0563(7) -0.0137(5) -0.0014(5) -0.0008(5) C1 0.0387(9) 0.0404(10) 0.0301(8) 0.0055(7) 0.0008(7) -0.0101(7) C2 0.0309(8) 0.0423(9) 0.0389(9) -0.0020(7) 0.0093(7) -0.0062(7) C3 0.0253(8) 0.0454(10) 0.0401(9) 0.0033(8) -0.0027(7) -0.0052(7) C4 0.0381(9) 0.0406(10) 0.0322(8) -0.0043(7) -0.0007(7) -0.0105(7) C5 0.0372(9) 0.0323(9) 0.0414(9) -0.0013(7) 0.0015(7) -0.0047(7) C6 0.0299(8) 0.0303(8) 0.0298(8) 0.0003(6) -0.0036(6) -0.0005(6) C7 0.0340(8) 0.0339(9) 0.0296(8) 0.0055(7) -0.0054(6) -0.0043(7) C8 0.0325(8) 0.0446(9) 0.0245(7) 0.0020(7) 0.0008(6) -0.0078(7) C9 0.0234(7) 0.0398(8) 0.0271(7) -0.0015(6) 0.0010(6) -0.0021(6) C10 0.0243(7) 0.0317(8) 0.0251(7) -0.0001(6) -0.0014(6) -0.0025(6) C11 0.0241(7) 0.0315(8) 0.0243(7) -0.0002(6) -0.0008(6) 0.0009(6) C12 0.0255(7) 0.0420(9) 0.0263(7) -0.0012(6) 0.0003(6) 0.0044(6) C13 0.0281(8) 0.0381(9) 0.0261(7) -0.0006(6) 0.0021(6) 0.0006(6) C14 0.0452(10) 0.0405(9) 0.0250(7) 0.0016(7) -0.0087(7) -0.0051(8) C15 0.0254(7) 0.0427(9) 0.0295(8) 0.0000(7) -0.0024(6) 0.0001(7) C16 0.0254(7) 0.0415(9) 0.0261(7) 0.0004(6) 0.0005(6) -0.0013(6) B1 0.0320(9) 0.0302(9) 0.0424(10) 0.0001(8) 0.0038(8) 0.0008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.0357(17) . ? Fe1 C6 2.0417(16) . ? Fe1 C10 2.0424(15) . ? Fe1 C9 2.0440(16) . ? Fe1 C2 2.0446(17) . ? Fe1 C5 2.0496(18) . ? Fe1 C7 2.0504(17) . ? Fe1 C4 2.0510(17) . ? Fe1 C3 2.0528(17) . ? Fe1 C8 2.0556(16) . ? F1 B1 1.386(2) . ? F2 B1 1.367(2) . ? F3 B1 1.412(2) . ? F4 B1 1.385(2) . ? N14 C14 1.4929(19) . ? N14 C15 1.496(2) . ? N14 C13 1.502(2) . ? C1 C5 1.419(3) . ? C1 C2 1.425(3) . ? C2 C3 1.425(2) . ? C3 C4 1.417(3) . ? C4 C5 1.429(3) . ? C6 C7 1.432(2) . ? C6 C10 1.433(2) . ? C7 C8 1.418(3) . ? C8 C9 1.428(2) . ? C9 C10 1.438(2) . ? C10 C11 1.504(2) . ? C11 C12 1.530(2) . ? C11 C16 1.534(2) . ? C12 C13 1.520(2) . ? C15 C16 1.520(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C6 121.65(7) . . ? C1 Fe1 C10 104.54(7) . . ? C6 Fe1 C10 41.08(6) . . ? C1 Fe1 C9 120.30(7) . . ? C6 Fe1 C9 68.85(7) . . ? C10 Fe1 C9 41.20(6) . . ? C1 Fe1 C2 40.89(8) . . ? C6 Fe1 C2 106.10(7) . . ? C10 Fe1 C2 119.55(7) . . ? C9 Fe1 C2 155.92(7) . . ? C1 Fe1 C5 40.64(7) . . ? C6 Fe1 C5 158.25(7) . . ? C10 Fe1 C5 121.75(7) . . ? C9 Fe1 C5 106.95(7) . . ? C2 Fe1 C5 68.57(8) . . ? C1 Fe1 C7 159.39(7) . . ? C6 Fe1 C7 40.98(7) . . ? C10 Fe1 C7 69.17(6) . . ? C9 Fe1 C7 68.62(7) . . ? C2 Fe1 C7 123.88(7) . . ? C5 Fe1 C7 159.22(7) . . ? C1 Fe1 C4 68.46(7) . . ? C6 Fe1 C4 158.76(7) . . ? C10 Fe1 C4 159.75(7) . . ? C9 Fe1 C4 124.62(7) . . ? C2 Fe1 C4 68.37(7) . . ? C5 Fe1 C4 40.78(7) . . ? C7 Fe1 C4 123.88(7) . . ? C1 Fe1 C3 68.53(7) . . ? C6 Fe1 C3 122.17(7) . . ? C10 Fe1 C3 156.56(7) . . ? C9 Fe1 C3 161.64(7) . . ? C2 Fe1 C3 40.71(7) . . ? C5 Fe1 C3 68.39(8) . . ? C7 Fe1 C3 109.05(7) . . ? C4 Fe1 C3 40.41(8) . . ? C1 Fe1 C8 157.39(8) . . ? C6 Fe1 C8 68.50(7) . . ? C10 Fe1 C8 69.00(6) . . ? C9 Fe1 C8 40.78(6) . . ? C2 Fe1 C8 161.20(7) . . ? C5 Fe1 C8 123.12(7) . . ? C7 Fe1 C8 40.42(7) . . ? C4 Fe1 C8 109.77(7) . . ? C3 Fe1 C8 125.73(7) . . ? C14 N14 C15 111.55(13) . . ? C14 N14 C13 111.76(13) . . ? C15 N14 C13 111.19(12) . . ? C5 C1 C2 108.36(16) . . ? C5 C1 Fe1 70.21(10) . . ? C2 C1 Fe1 69.89(10) . . ? C3 C2 C1 107.70(16) . . ? C3 C2 Fe1 69.95(10) . . ? C1 C2 Fe1 69.22(10) . . ? C4 C3 C2 108.08(16) . . ? C4 C3 Fe1 69.72(10) . . ? C2 C3 Fe1 69.33(10) . . ? C3 C4 C5 108.20(16) . . ? C3 C4 Fe1 69.86(10) . . ? C5 C4 Fe1 69.56(10) . . ? C1 C5 C4 107.66(16) . . ? C1 C5 Fe1 69.15(10) . . ? C4 C5 Fe1 69.66(10) . . ? C7 C6 C10 108.36(14) . . ? C7 C6 Fe1 69.84(9) . . ? C10 C6 Fe1 69.49(9) . . ? C8 C7 C6 107.97(14) . . ? C8 C7 Fe1 69.98(10) . . ? C6 C7 Fe1 69.18(9) . . ? C7 C8 C9 108.34(14) . . ? C7 C8 Fe1 69.60(9) . . ? C9 C8 Fe1 69.18(9) . . ? C8 C9 C10 108.18(15) . . ? C8 C9 Fe1 70.05(9) . . ? C10 C9 Fe1 69.34(9) . . ? C6 C10 C9 107.15(13) . . ? C6 C10 C11 127.69(14) . . ? C9 C10 C11 125.16(14) . . ? C6 C10 Fe1 69.43(9) . . ? C9 C10 Fe1 69.46(9) . . ? C11 C10 Fe1 126.42(11) . . ? C10 C11 C12 112.00(12) . . ? C10 C11 C16 111.18(13) . . ? C12 C11 C16 109.15(13) . . ? C13 C12 C11 112.20(13) . . ? N14 C13 C12 109.93(13) . . ? N14 C15 C16 110.37(13) . . ? C15 C16 C11 111.26(13) . . ? F2 B1 F4 110.24(16) . . ? F2 B1 F1 110.63(16) . . ? F4 B1 F1 109.47(16) . . ? F2 B1 F3 110.46(16) . . ? F4 B1 F3 108.75(15) . . ? F1 B1 F3 107.22(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.473 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.133 #================================================================= data_sjf130-3 _database_code_depnum_ccdc_archive 'CCDC 219615' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 B F4 Fe N' _chemical_formula_weight 344.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8882(2) _cell_length_b 13.1010(2) _cell_length_c 20.0636(4) _cell_angle_alpha 74.6948(6) _cell_angle_beta 74.7805(6) _cell_angle_gamma 70.9655(6) _cell_volume 3030.53(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description orange _exptl_crystal_colour prism _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7758 _exptl_absorpt_correction_T_max 0.8527 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54668 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11880 _reflns_number_gt 9345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+1.1004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11880 _refine_ls_number_parameters 874 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.34951(2) 0.14397(2) 0.116669(15) 0.02729(9) Uani 1 1 d . . . Fe2 Fe -0.13863(2) 0.37322(2) -0.147224(16) 0.02767(9) Uani 1 1 d . . . Fe3 Fe 0.36348(2) 0.35939(2) -0.141560(16) 0.02795(9) Uani 1 1 d . . . Fe4 Fe 0.13965(2) 0.15340(2) 0.118329(15) 0.02697(9) Uani 1 1 d . . . F9 F -0.26845(15) -0.23153(14) 0.33057(9) 0.0696(5) Uani 1 1 d . . . F10 F -0.15186(13) -0.22830(13) 0.39634(10) 0.0739(5) Uani 1 1 d . . . F11 F -0.25449(11) -0.06772(11) 0.34229(8) 0.0514(4) Uani 1 1 d . . . F12 F -0.33950(13) -0.17451(13) 0.43343(8) 0.0612(4) Uani 1 1 d . . . F1A F 0.2618(4) 0.6902(4) -0.4535(2) 0.1119(15) Uani 0.50 1 d P A 2 F2A F 0.3525(10) 0.5973(10) -0.3648(7) 0.090(3) Uani 0.50 1 d P A 2 F3A F 0.2994(4) 0.7819(4) -0.3886(4) 0.093(2) Uani 0.50 1 d P A 2 F4A F 0.1696(3) 0.6882(4) -0.3430(2) 0.0654(11) Uani 0.50 1 d P A 2 F5A F -0.9055(6) 0.1613(8) 0.3896(6) 0.108(4) Uani 0.30 1 d P B 1 F6A F -0.7401(5) 0.1814(6) 0.3289(3) 0.0779(19) Uani 0.30 1 d P B 1 F7A F -0.7849(5) 0.0176(5) 0.3494(4) 0.0756(18) Uani 0.30 1 d P B 1 F8A F -0.7432(8) 0.0736(7) 0.4332(4) 0.082(3) Uani 0.30 1 d P B 1 F13A F 0.6834(10) 0.4481(9) -0.3377(5) 0.081(3) Uani 0.50 1 d P C 1 F14A F 0.8285(4) 0.4819(4) -0.4274(3) 0.0740(14) Uani 0.50 1 d P C 2 F15A F 0.7653(8) 0.3291(7) -0.3868(4) 0.0580(17) Uani 0.50 1 d P C 1 F16A F 0.6545(4) 0.4891(3) -0.4317(2) 0.0578(11) Uani 0.50 1 d P C 2 F1B F 0.3233(9) 0.5844(10) -0.3762(7) 0.080(3) Uani 0.50 1 d P A 1 F2B F 0.3194(5) 0.7583(4) -0.4263(3) 0.0769(17) Uani 0.50 1 d P A 1 F3B F 0.2587(3) 0.7158(3) -0.31097(18) 0.0718(9) Uani 0.50 1 d P A 1 F4B F 0.1577(4) 0.7140(4) -0.3853(3) 0.0698(13) Uani 0.50 1 d P A 1 F5B F -0.8750(2) 0.1760(2) 0.34833(14) 0.0540(7) Uani 0.70 1 d P B 2 F6B F -0.68888(16) 0.08567(19) 0.32844(10) 0.0459(5) Uani 0.70 1 d P B 2 F7B F -0.81424(19) 0.00144(18) 0.40583(15) 0.0598(6) Uani 0.70 1 d P B 2 F8B F -0.7735(2) 0.1396(2) 0.43273(16) 0.0524(7) Uani 0.70 1 d P B 2 F13B F 0.7047(10) 0.4691(8) -0.3287(5) 0.0565(19) Uani 0.50 1 d P C 2 F14B F 0.8620(4) 0.4168(5) -0.3965(3) 0.0944(16) Uani 0.50 1 d P C 1 F15B F 0.7592(8) 0.3276(8) -0.4126(5) 0.083(3) Uani 0.50 1 d P C 2 F16B F 0.7232(7) 0.5082(4) -0.4534(2) 0.135(3) Uani 0.50 1 d P C 1 N1 N -0.54874(14) 0.18062(13) 0.36830(9) 0.0311(4) Uani 1 1 d . . . H57 H -0.6085 0.1629 0.3608 0.037 Uiso 1 1 calc R . . N2 N 0.02714(16) 0.58626(14) -0.38285(10) 0.0399(4) Uani 1 1 d . . . H58 H 0.0546 0.6391 -0.3757 0.048 Uiso 1 1 calc R . . N3 N 0.55030(15) 0.29703(15) -0.38984(10) 0.0386(4) Uani 1 1 d . . . H59 H 0.6171 0.3164 -0.4014 0.046 Uiso 1 1 calc R . . N4 N -0.05209(14) -0.03422(14) 0.35522(9) 0.0334(4) Uani 1 1 d . . . H60 H -0.1095 -0.0580 0.3499 0.040 Uiso 1 1 calc R . . C1 C -0.43433(16) 0.26871(15) 0.17135(11) 0.0288(4) Uani 1 1 d . . . C2 C -0.46092(17) 0.29632(15) 0.10301(11) 0.0312(5) Uani 1 1 d . . . H2 H -0.5334 0.3126 0.0932 0.037 Uiso 1 1 calc R . . C3 C -0.36020(17) 0.29524(16) 0.05202(11) 0.0330(5) Uani 1 1 d . . . H3 H -0.3537 0.3112 0.0023 0.040 Uiso 1 1 calc R . . C4 C -0.27105(18) 0.26598(16) 0.08892(11) 0.0320(5) Uani 1 1 d . . . H4 H -0.1944 0.2583 0.0680 0.038 Uiso 1 1 calc R . . C5 C -0.31622(17) 0.25021(16) 0.16220(11) 0.0309(5) Uani 1 1 d . . . H5 H -0.2752 0.2307 0.1988 0.037 Uiso 1 1 calc R . . C6 C -0.51744(17) 0.26642(17) 0.23971(11) 0.0327(5) Uani 1 1 d . . . H6A H -0.5813 0.2446 0.2348 0.039 Uiso 1 1 calc R . . H6B H -0.5465 0.3412 0.2507 0.039 Uiso 1 1 calc R . . C7 C -0.46578(17) 0.18695(17) 0.29977(11) 0.0336(5) Uani 1 1 d . . . H7A H -0.4343 0.1128 0.2879 0.040 Uiso 1 1 calc R . . H7B H -0.4035 0.2103 0.3055 0.040 Uiso 1 1 calc R . . C8 C -0.4988(2) 0.09138(19) 0.42358(12) 0.0439(6) Uani 1 1 d . . . H8A H -0.4374 0.1092 0.4340 0.066 Uiso 1 1 calc R . . H8B H -0.4702 0.0217 0.4068 0.066 Uiso 1 1 calc R . . H8C H -0.5561 0.0844 0.4664 0.066 Uiso 1 1 calc R . . C9 C -0.5942(2) 0.28711(18) 0.39327(13) 0.0459(6) Uani 1 1 d . . . H9A H -0.6428 0.2769 0.4397 0.069 Uiso 1 1 calc R . . H9B H -0.6373 0.3424 0.3598 0.069 Uiso 1 1 calc R . . H9C H -0.5322 0.3121 0.3967 0.069 Uiso 1 1 calc R . . C10 C -0.4038(2) 0.04017(18) 0.08289(15) 0.0493(7) Uani 1 1 d . . . H10 H -0.4627 0.0614 0.0575 0.059 Uiso 1 1 calc R . . C11 C -0.2898(2) 0.02979(19) 0.05370(14) 0.0467(6) Uani 1 1 d . . . H11 H -0.2581 0.0427 0.0049 0.056 Uiso 1 1 calc R . . C12 C -0.2314(2) -0.00256(18) 0.10852(16) 0.0507(7) Uani 1 1 d . . . H12 H -0.1531 -0.0150 0.1034 0.061 Uiso 1 1 calc R . . C13 C -0.3069(3) -0.01372(18) 0.17228(14) 0.0533(7) Uani 1 1 d . . . H13 H -0.2889 -0.0355 0.2179 0.064 Uiso 1 1 calc R . . C14 C -0.4146(2) 0.01302(19) 0.15713(15) 0.0561(8) Uani 1 1 d . . . H14 H -0.4821 0.0129 0.1906 0.067 Uiso 1 1 calc R . . C15 C -0.10866(17) 0.52450(16) -0.18687(11) 0.0319(5) Uani 1 1 d . . . C16 C -0.08192(19) 0.48093(16) -0.11846(11) 0.0342(5) Uani 1 1 d . . . H16 H -0.0107 0.4664 -0.1071 0.041 Uiso 1 1 calc R . . C17 C -0.18002(19) 0.46301(17) -0.07013(12) 0.0379(5) Uani 1 1 d . . . H17 H -0.1857 0.4349 -0.0210 0.046 Uiso 1 1 calc R . . C18 C -0.26771(19) 0.49434(17) -0.10795(12) 0.0388(5) Uani 1 1 d . . . H18 H -0.3424 0.4907 -0.0887 0.047 Uiso 1 1 calc R . . C19 C -0.22394(17) 0.53243(16) -0.18012(12) 0.0354(5) Uani 1 1 d . . . H19 H -0.2646 0.5586 -0.2173 0.043 Uiso 1 1 calc R . . C20 C -0.02829(18) 0.55834(18) -0.25194(11) 0.0365(5) Uani 1 1 d . . . H20A H 0.0464 0.5051 -0.2507 0.044 Uiso 1 1 calc R . . H20B H -0.0217 0.6314 -0.2515 0.044 Uiso 1 1 calc R . . C21 C -0.06219(18) 0.56447(18) -0.31970(11) 0.0371(5) Uani 1 1 d . . . H21A H -0.0766 0.4942 -0.3184 0.044 Uiso 1 1 calc R . . H21B H -0.1324 0.6240 -0.3241 0.044 Uiso 1 1 calc R . . C22 C -0.0177(2) 0.6313(2) -0.44879(13) 0.0583(7) Uani 1 1 d . . . H22A H 0.0429 0.6440 -0.4884 0.088 Uiso 1 1 calc R . . H22B H -0.0756 0.7010 -0.4447 0.088 Uiso 1 1 calc R . . H22C H -0.0502 0.5786 -0.4569 0.088 Uiso 1 1 calc R . . C23 C 0.1225(2) 0.4863(2) -0.39064(15) 0.0618(8) Uani 1 1 d . . . H23A H 0.0964 0.4293 -0.3992 0.093 Uiso 1 1 calc R . . H23B H 0.1531 0.4589 -0.3474 0.093 Uiso 1 1 calc R . . H23C H 0.1807 0.5047 -0.4304 0.093 Uiso 1 1 calc R . . C24 C -0.1581(2) 0.28164(17) -0.20889(12) 0.0401(5) Uani 1 1 d . . . H24 H -0.1992 0.3086 -0.2459 0.048 Uiso 1 1 calc R . . C25 C -0.04256(19) 0.27233(17) -0.21574(13) 0.0394(5) Uani 1 1 d . . . H25 H 0.0070 0.2920 -0.2581 0.047 Uiso 1 1 calc R . . C26 C -0.01471(18) 0.22837(16) -0.14798(13) 0.0372(5) Uani 1 1 d . . . H26 H 0.0568 0.2133 -0.1369 0.045 Uiso 1 1 calc R . . C27 C -0.11296(19) 0.21094(16) -0.09955(12) 0.0369(5) Uani 1 1 d . . . H27 H -0.1186 0.1823 -0.0504 0.044 Uiso 1 1 calc R . . C28 C -0.20072(19) 0.24360(17) -0.13730(13) 0.0385(5) Uani 1 1 d . . . H28 H -0.2755 0.2405 -0.1179 0.046 Uiso 1 1 calc R . . C29 C 0.52180(16) 0.29276(17) -0.19360(12) 0.0330(5) Uani 1 1 d . . . C30 C 0.50130(17) 0.23104(18) -0.12379(12) 0.0358(5) Uani 1 1 d . . . H30 H 0.5045 0.1550 -0.1115 0.043 Uiso 1 1 calc R . . C31 C 0.47521(17) 0.30247(19) -0.07577(12) 0.0373(5) Uani 1 1 d . . . H31 H 0.4579 0.2826 -0.0259 0.045 Uiso 1 1 calc R . . C32 C 0.47949(18) 0.40879(19) -0.11542(12) 0.0396(5) Uani 1 1 d . . . H32 H 0.4656 0.4726 -0.0968 0.048 Uiso 1 1 calc R . . C33 C 0.50828(17) 0.40279(18) -0.18793(12) 0.0356(5) Uani 1 1 d . . . H33 H 0.5170 0.4621 -0.2262 0.043 Uiso 1 1 calc R . . C34 C 0.55963(18) 0.24716(18) -0.26028(12) 0.0384(5) Uani 1 1 d . . . H34A H 0.5506 0.1719 -0.2495 0.046 Uiso 1 1 calc R . . H34B H 0.6401 0.2419 -0.2783 0.046 Uiso 1 1 calc R . . C35 C 0.49367(18) 0.31848(18) -0.31714(11) 0.0384(5) Uani 1 1 d . . . H35A H 0.4191 0.3050 -0.3055 0.046 Uiso 1 1 calc R . . H35B H 0.4821 0.3969 -0.3170 0.046 Uiso 1 1 calc R . . C36 C 0.4803(2) 0.36845(19) -0.44232(12) 0.0457(6) Uani 1 1 d . . . H36A H 0.5229 0.3619 -0.4900 0.069 Uiso 1 1 calc R . . H36B H 0.4598 0.4452 -0.4371 0.069 Uiso 1 1 calc R . . H36C H 0.4124 0.3452 -0.4344 0.069 Uiso 1 1 calc R . . C37 C 0.5782(2) 0.1797(2) -0.39482(15) 0.0558(7) Uani 1 1 d . . . H37A H 0.5100 0.1553 -0.3797 0.084 Uiso 1 1 calc R . . H37B H 0.6317 0.1348 -0.3644 0.084 Uiso 1 1 calc R . . H37C H 0.6115 0.1716 -0.4437 0.084 Uiso 1 1 calc R . . C38 C 0.24191(18) 0.4567(2) -0.19664(13) 0.0432(6) Uani 1 1 d . . . H38 H 0.2527 0.5068 -0.2400 0.052 Uiso 1 1 calc R . . C39 C 0.24722(17) 0.34419(19) -0.18860(12) 0.0383(5) Uani 1 1 d . . . H39 H 0.2616 0.3058 -0.2256 0.046 Uiso 1 1 calc R . . C40 C 0.22723(17) 0.29940(18) -0.11558(12) 0.0353(5) Uani 1 1 d . . . H40 H 0.2264 0.2254 -0.0951 0.042 Uiso 1 1 calc R . . C41 C 0.20867(17) 0.38382(18) -0.07836(12) 0.0362(5) Uani 1 1 d . . . H41 H 0.1930 0.3764 -0.0286 0.043 Uiso 1 1 calc R . . C42 C 0.21761(18) 0.48118(18) -0.12826(13) 0.0413(6) Uani 1 1 d . . . H42 H 0.2089 0.5506 -0.1179 0.050 Uiso 1 1 calc R . . C43 C -0.00865(16) 0.11400(16) 0.16115(11) 0.0292(4) Uani 1 1 d . . . C44 C 0.03133(17) 0.09493(17) 0.09064(11) 0.0319(5) Uani 1 1 d . . . H44 H 0.0484 0.0264 0.0767 0.038 Uiso 1 1 calc R . . C45 C 0.04111(17) 0.19623(17) 0.04498(12) 0.0341(5) Uani 1 1 d . . . H45 H 0.0658 0.2071 -0.0047 0.041 Uiso 1 1 calc R . . C46 C 0.00762(16) 0.27829(17) 0.08645(12) 0.0333(5) Uani 1 1 d . . . H46 H 0.0063 0.3535 0.0695 0.040 Uiso 1 1 calc R . . C47 C -0.02367(16) 0.22777(16) 0.15806(11) 0.0311(5) Uani 1 1 d . . . H47 H -0.0500 0.2638 0.1971 0.037 Uiso 1 1 calc R . . C48 C -0.03405(18) 0.02798(17) 0.22464(11) 0.0343(5) Uani 1 1 d . . . H48A H 0.0221 -0.0434 0.2194 0.041 Uiso 1 1 calc R . . H48B H -0.1084 0.0193 0.2268 0.041 Uiso 1 1 calc R . . C49 C -0.03356(18) 0.05630(16) 0.29302(11) 0.0322(5) Uani 1 1 d . . . H49A H 0.0391 0.0694 0.2900 0.039 Uiso 1 1 calc R . . H49B H -0.0931 0.1251 0.3000 0.039 Uiso 1 1 calc R . . C50 C -0.0890(2) 0.0064(2) 0.42271(12) 0.0482(6) Uani 1 1 d . . . H50A H -0.1004 -0.0544 0.4620 0.072 Uiso 1 1 calc R . . H50B H -0.1593 0.0651 0.4216 0.072 Uiso 1 1 calc R . . H50C H -0.0316 0.0351 0.4289 0.072 Uiso 1 1 calc R . . C51 C 0.0480(2) -0.13074(18) 0.35861(13) 0.0438(6) Uani 1 1 d . . . H51A H 0.1091 -0.1093 0.3667 0.066 Uiso 1 1 calc R . . H51B H 0.0712 -0.1569 0.3141 0.066 Uiso 1 1 calc R . . H51C H 0.0299 -0.1897 0.3973 0.066 Uiso 1 1 calc R . . C52 C 0.24047(18) 0.17441(19) 0.17484(12) 0.0373(5) Uani 1 1 d . . . H52 H 0.2166 0.2131 0.2125 0.045 Uiso 1 1 calc R . . C53 C 0.25315(17) 0.06058(18) 0.18085(12) 0.0384(5) Uani 1 1 d . . . H53 H 0.2392 0.0099 0.2235 0.046 Uiso 1 1 calc R . . C54 C 0.29011(17) 0.03570(18) 0.11264(13) 0.0382(5) Uani 1 1 d . . . H54 H 0.3053 -0.0345 0.1014 0.046 Uiso 1 1 calc R . . C55 C 0.30049(17) 0.13428(18) 0.06380(12) 0.0351(5) Uani 1 1 d . . . H55 H 0.3238 0.1417 0.0142 0.042 Uiso 1 1 calc R . . C56 C 0.26989(17) 0.21969(18) 0.10245(12) 0.0349(5) Uani 1 1 d . . . H56 H 0.2693 0.2943 0.0831 0.042 Uiso 1 1 calc R . . B1 B 0.2695(2) 0.6899(2) -0.38055(17) 0.0495(7) Uani 1 1 d . . . B2 B -0.7899(2) 0.1014(2) 0.37826(15) 0.0418(6) Uani 1 1 d . . . B3 B -0.2546(2) -0.1768(2) 0.37559(15) 0.0400(6) Uani 1 1 d . . . B4 B 0.7462(3) 0.4354(2) -0.39690(16) 0.0477(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02426(16) 0.02619(15) 0.03266(18) -0.00649(12) -0.00607(13) -0.00755(12) Fe2 0.02453(16) 0.02483(15) 0.03515(18) -0.00776(12) -0.00709(13) -0.00625(12) Fe3 0.02300(16) 0.02891(16) 0.03376(18) -0.00563(12) -0.00679(12) -0.00893(12) Fe4 0.02186(16) 0.02756(16) 0.03207(18) -0.00582(12) -0.00600(12) -0.00699(12) F9 0.0859(12) 0.0800(11) 0.0625(10) -0.0351(9) -0.0053(9) -0.0389(10) F10 0.0550(10) 0.0495(9) 0.1216(15) -0.0114(9) -0.0335(10) -0.0116(8) F11 0.0486(8) 0.0490(8) 0.0585(9) -0.0003(7) -0.0115(7) -0.0232(7) F12 0.0657(10) 0.0690(10) 0.0485(9) -0.0153(7) 0.0117(8) -0.0327(8) F1A 0.119(4) 0.163(4) 0.070(3) -0.030(3) -0.009(3) -0.063(3) F2A 0.062(4) 0.054(4) 0.114(8) 0.010(4) 0.000(4) 0.003(3) F3A 0.054(3) 0.049(2) 0.194(7) -0.017(4) -0.057(4) -0.019(2) F4A 0.040(2) 0.066(3) 0.089(3) -0.028(2) 0.010(2) -0.0202(18) F5A 0.040(4) 0.109(7) 0.192(11) -0.079(8) 0.008(6) -0.026(4) F6A 0.082(4) 0.111(5) 0.058(4) 0.021(3) -0.029(3) -0.066(4) F7A 0.072(4) 0.065(4) 0.110(5) -0.039(4) -0.051(4) -0.001(3) F8A 0.105(7) 0.131(7) 0.034(3) 0.002(5) -0.018(4) -0.075(6) F13A 0.077(5) 0.058(4) 0.066(6) 0.002(3) 0.030(4) -0.007(3) F14A 0.068(3) 0.089(3) 0.073(3) -0.021(2) 0.019(2) -0.053(3) F15A 0.058(3) 0.036(3) 0.081(4) -0.019(2) -0.026(3) 0.0015(18) F16A 0.074(3) 0.0422(18) 0.072(3) -0.0086(19) -0.046(2) -0.0125(18) F1B 0.087(7) 0.055(3) 0.082(3) -0.031(3) -0.015(4) 0.015(4) F2B 0.057(2) 0.067(3) 0.085(3) 0.010(2) 0.010(2) -0.027(2) F3B 0.079(2) 0.085(2) 0.061(2) -0.0370(19) -0.0107(18) -0.0195(19) F4B 0.051(2) 0.062(2) 0.109(4) -0.010(3) -0.027(3) -0.0276(18) F5B 0.0505(18) 0.0542(13) 0.0568(16) -0.0072(13) -0.0216(13) -0.0080(13) F6B 0.0439(11) 0.0619(13) 0.0383(11) -0.0152(10) -0.0035(9) -0.0222(10) F7B 0.0537(14) 0.0464(12) 0.0799(17) -0.0041(12) -0.0086(13) -0.0244(10) F8B 0.0464(14) 0.0718(18) 0.0489(15) -0.0273(16) -0.0080(11) -0.0180(14) F13B 0.078(4) 0.049(4) 0.031(2) -0.005(2) -0.014(2) -0.002(3) F14B 0.067(3) 0.126(4) 0.122(5) -0.074(4) 0.006(3) -0.049(3) F15B 0.038(3) 0.064(3) 0.158(8) -0.061(5) 0.002(4) -0.015(2) F16B 0.229(9) 0.072(4) 0.042(3) -0.012(2) -0.022(4) 0.038(4) N1 0.0281(9) 0.0330(9) 0.0308(10) -0.0069(7) -0.0020(7) -0.0090(7) N2 0.0454(11) 0.0345(10) 0.0391(11) -0.0086(8) -0.0009(9) -0.0149(8) N3 0.0329(10) 0.0434(10) 0.0427(11) -0.0174(9) -0.0025(8) -0.0112(8) N4 0.0320(9) 0.0358(9) 0.0333(10) -0.0036(8) -0.0042(8) -0.0143(8) C1 0.0282(11) 0.0250(10) 0.0335(12) -0.0075(8) -0.0047(9) -0.0073(8) C2 0.0285(11) 0.0262(10) 0.0382(12) -0.0051(9) -0.0084(9) -0.0059(8) C3 0.0363(12) 0.0287(10) 0.0332(12) -0.0043(9) -0.0055(9) -0.0103(9) C4 0.0296(11) 0.0331(11) 0.0352(12) -0.0075(9) -0.0027(9) -0.0132(9) C5 0.0304(11) 0.0301(10) 0.0353(12) -0.0063(9) -0.0082(9) -0.0110(9) C6 0.0271(11) 0.0345(11) 0.0347(12) -0.0073(9) -0.0050(9) -0.0063(9) C7 0.0284(11) 0.0373(11) 0.0304(12) -0.0079(9) -0.0004(9) -0.0061(9) C8 0.0443(14) 0.0417(13) 0.0350(13) -0.0001(10) -0.0064(11) -0.0045(10) C9 0.0552(15) 0.0370(12) 0.0381(13) -0.0146(10) -0.0002(11) -0.0041(11) C10 0.0502(15) 0.0344(12) 0.077(2) -0.0151(12) -0.0308(14) -0.0114(11) C11 0.0575(16) 0.0394(13) 0.0461(15) -0.0188(11) -0.0005(12) -0.0161(11) C12 0.0391(14) 0.0324(12) 0.085(2) -0.0217(12) -0.0197(14) -0.0012(10) C13 0.085(2) 0.0268(12) 0.0528(16) -0.0025(10) -0.0322(15) -0.0106(12) C14 0.0589(17) 0.0342(13) 0.072(2) -0.0166(12) 0.0171(15) -0.0270(12) C15 0.0306(11) 0.0261(10) 0.0403(13) -0.0077(9) -0.0071(9) -0.0084(8) C16 0.0366(12) 0.0292(11) 0.0416(13) -0.0106(9) -0.0109(10) -0.0098(9) C17 0.0465(14) 0.0304(11) 0.0382(13) -0.0117(9) -0.0032(11) -0.0124(10) C18 0.0311(12) 0.0276(11) 0.0524(15) -0.0115(10) 0.0002(10) -0.0049(9) C19 0.0296(11) 0.0269(10) 0.0482(14) -0.0054(9) -0.0100(10) -0.0053(9) C20 0.0335(12) 0.0376(12) 0.0426(13) -0.0069(10) -0.0070(10) -0.0162(9) C21 0.0358(12) 0.0352(11) 0.0405(13) -0.0051(9) -0.0046(10) -0.0143(10) C22 0.076(2) 0.0501(15) 0.0377(15) -0.0067(11) -0.0065(13) -0.0075(14) C23 0.0548(17) 0.0532(16) 0.0612(18) -0.0178(13) 0.0003(14) 0.0024(13) C24 0.0476(14) 0.0342(11) 0.0451(14) -0.0123(10) -0.0206(11) -0.0072(10) C25 0.0418(13) 0.0310(11) 0.0439(14) -0.0152(10) 0.0022(11) -0.0102(10) C26 0.0301(11) 0.0270(10) 0.0571(15) -0.0138(10) -0.0143(11) -0.0023(9) C27 0.0449(13) 0.0266(10) 0.0409(13) -0.0070(9) -0.0104(11) -0.0102(9) C28 0.0349(12) 0.0322(11) 0.0546(15) -0.0152(10) -0.0077(11) -0.0129(9) C29 0.0220(10) 0.0367(11) 0.0426(13) -0.0086(9) -0.0080(9) -0.0090(9) C30 0.0232(11) 0.0375(12) 0.0460(14) -0.0023(10) -0.0133(10) -0.0066(9) C31 0.0267(11) 0.0503(13) 0.0379(13) -0.0089(10) -0.0106(10) -0.0110(10) C32 0.0299(12) 0.0498(13) 0.0493(15) -0.0180(11) -0.0076(10) -0.0178(10) C33 0.0298(11) 0.0390(12) 0.0422(13) -0.0080(10) -0.0042(10) -0.0172(9) C34 0.0329(12) 0.0358(11) 0.0438(14) -0.0111(10) -0.0054(10) -0.0049(9) C35 0.0332(12) 0.0417(12) 0.0380(13) -0.0143(10) -0.0013(10) -0.0065(10) C36 0.0523(15) 0.0430(13) 0.0400(14) -0.0081(10) -0.0098(11) -0.0102(11) C37 0.0653(18) 0.0434(14) 0.0582(17) -0.0236(12) -0.0197(14) 0.0026(12) C38 0.0290(12) 0.0514(14) 0.0440(14) 0.0056(11) -0.0118(10) -0.0123(10) C39 0.0252(11) 0.0568(14) 0.0385(13) -0.0150(11) -0.0069(9) -0.0135(10) C40 0.0253(11) 0.0378(12) 0.0457(14) -0.0057(10) -0.0076(10) -0.0141(9) C41 0.0257(11) 0.0467(13) 0.0363(13) -0.0092(10) -0.0050(9) -0.0103(9) C42 0.0266(11) 0.0349(12) 0.0612(16) -0.0116(11) -0.0103(11) -0.0038(9) C43 0.0237(10) 0.0332(11) 0.0329(12) -0.0071(9) -0.0052(9) -0.0106(8) C44 0.0258(11) 0.0360(11) 0.0379(12) -0.0110(9) -0.0076(9) -0.0098(9) C45 0.0258(11) 0.0449(12) 0.0331(12) -0.0057(9) -0.0075(9) -0.0117(9) C46 0.0226(10) 0.0301(11) 0.0443(13) -0.0008(9) -0.0103(9) -0.0056(8) C47 0.0219(10) 0.0335(11) 0.0381(12) -0.0100(9) -0.0038(9) -0.0071(8) C48 0.0365(12) 0.0358(11) 0.0354(12) -0.0067(9) -0.0056(10) -0.0176(9) C49 0.0325(11) 0.0296(10) 0.0331(12) -0.0041(9) -0.0023(9) -0.0117(9) C50 0.0509(15) 0.0522(14) 0.0337(13) -0.0088(11) 0.0032(11) -0.0127(12) C51 0.0473(14) 0.0360(12) 0.0457(14) -0.0054(10) -0.0142(11) -0.0065(10) C52 0.0283(11) 0.0482(13) 0.0399(13) -0.0123(10) -0.0117(10) -0.0097(10) C53 0.0277(11) 0.0428(12) 0.0398(13) 0.0012(10) -0.0107(10) -0.0074(9) C54 0.0246(11) 0.0325(11) 0.0564(15) -0.0112(10) -0.0112(10) -0.0018(9) C55 0.0233(10) 0.0437(12) 0.0387(13) -0.0108(10) -0.0056(9) -0.0079(9) C56 0.0251(11) 0.0374(11) 0.0456(14) -0.0054(10) -0.0103(10) -0.0122(9) B1 0.0407(16) 0.0418(16) 0.065(2) -0.0088(14) -0.0082(15) -0.0124(13) B2 0.0417(15) 0.0471(15) 0.0424(16) -0.0099(12) -0.0068(13) -0.0200(13) B3 0.0369(14) 0.0419(14) 0.0436(16) -0.0119(12) 0.0003(12) -0.0178(12) B4 0.0517(18) 0.0478(17) 0.0466(18) -0.0053(13) -0.0050(15) -0.0243(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C14 2.038(2) . ? Fe1 C10 2.039(2) . ? Fe1 C12 2.039(2) . ? Fe1 C11 2.040(2) . ? Fe1 C2 2.0418(19) . ? Fe1 C4 2.044(2) . ? Fe1 C13 2.044(2) . ? Fe1 C3 2.046(2) . ? Fe1 C1 2.055(2) . ? Fe1 C5 2.055(2) . ? Fe2 C19 2.038(2) . ? Fe2 C18 2.039(2) . ? Fe2 C25 2.042(2) . ? Fe2 C24 2.044(2) . ? Fe2 C26 2.044(2) . ? Fe2 C17 2.044(2) . ? Fe2 C27 2.044(2) . ? Fe2 C16 2.045(2) . ? Fe2 C28 2.047(2) . ? Fe2 C15 2.0532(19) . ? Fe3 C31 2.037(2) . ? Fe3 C32 2.038(2) . ? Fe3 C42 2.039(2) . ? Fe3 C41 2.040(2) . ? Fe3 C38 2.040(2) . ? Fe3 C33 2.043(2) . ? Fe3 C40 2.044(2) . ? Fe3 C30 2.044(2) . ? Fe3 C39 2.052(2) . ? Fe3 C29 2.053(2) . ? Fe4 C55 2.043(2) . ? Fe4 C44 2.043(2) . ? Fe4 C45 2.043(2) . ? Fe4 C54 2.044(2) . ? Fe4 C46 2.046(2) . ? Fe4 C53 2.047(2) . ? Fe4 C56 2.049(2) . ? Fe4 C43 2.0506(19) . ? Fe4 C47 2.051(2) . ? Fe4 C52 2.055(2) . ? F9 B3 1.369(3) . ? F10 B3 1.393(3) . ? F11 B3 1.409(3) . ? F12 B3 1.370(3) . ? F1A B1 1.492(5) . ? F2A B1 1.358(12) . ? F3A B1 1.339(6) . ? F4A B1 1.314(5) . ? F5A B2 1.429(8) . ? F6A B2 1.432(6) . ? F7A B2 1.346(6) . ? F8A B2 1.306(8) . ? F13A B4 1.267(11) . ? F14A B4 1.326(5) . ? F15A B4 1.301(9) . ? F16A B4 1.418(5) . ? F1B B1 1.320(12) . ? F2B B1 1.300(6) . ? F3B B1 1.484(4) . ? F4B B1 1.395(5) . ? F5B B2 1.362(4) . ? F6B B2 1.410(3) . ? F7B B2 1.383(3) . ? F8B B2 1.403(4) . ? F13B B4 1.461(10) . ? F14B B4 1.434(6) . ? F15B B4 1.474(9) . ? F16B B4 1.306(6) . ? N1 C8 1.487(3) . ? N1 C9 1.491(3) . ? N1 C7 1.506(3) . ? N2 C22 1.483(3) . ? N2 C23 1.486(3) . ? N2 C21 1.507(3) . ? N3 C37 1.484(3) . ? N3 C36 1.492(3) . ? N3 C35 1.504(3) . ? N4 C51 1.485(3) . ? N4 C50 1.490(3) . ? N4 C49 1.506(2) . ? C1 C2 1.426(3) . ? C1 C5 1.430(3) . ? C1 C6 1.502(3) . ? C2 C3 1.425(3) . ? C3 C4 1.423(3) . ? C4 C5 1.418(3) . ? C6 C7 1.512(3) . ? C10 C11 1.407(4) . ? C10 C14 1.417(4) . ? C11 C12 1.392(4) . ? C12 C13 1.395(4) . ? C13 C14 1.411(4) . ? C15 C16 1.427(3) . ? C15 C19 1.427(3) . ? C15 C20 1.503(3) . ? C16 C17 1.422(3) . ? C17 C18 1.416(3) . ? C18 C19 1.427(3) . ? C20 C21 1.509(3) . ? C24 C28 1.414(3) . ? C24 C25 1.427(3) . ? C25 C26 1.420(3) . ? C26 C27 1.423(3) . ? C27 C28 1.414(3) . ? C29 C30 1.426(3) . ? C29 C33 1.426(3) . ? C29 C34 1.508(3) . ? C30 C31 1.420(3) . ? C31 C32 1.421(3) . ? C32 C33 1.421(3) . ? C34 C35 1.525(3) . ? C38 C39 1.420(3) . ? C38 C42 1.423(3) . ? C39 C40 1.415(3) . ? C40 C41 1.417(3) . ? C41 C42 1.416(3) . ? C43 C47 1.426(3) . ? C43 C44 1.432(3) . ? C43 C48 1.505(3) . ? C44 C45 1.422(3) . ? C45 C46 1.420(3) . ? C46 C47 1.426(3) . ? C48 C49 1.515(3) . ? C52 C56 1.417(3) . ? C52 C53 1.422(3) . ? C53 C54 1.413(3) . ? C54 C55 1.422(3) . ? C55 C56 1.421(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Fe1 C10 40.69(11) . . ? C14 Fe1 C12 67.65(11) . . ? C10 Fe1 C12 67.66(10) . . ? C14 Fe1 C11 67.84(10) . . ? C10 Fe1 C11 40.36(10) . . ? C12 Fe1 C11 39.91(10) . . ? C14 Fe1 C2 116.84(10) . . ? C10 Fe1 C2 108.12(9) . . ? C12 Fe1 C2 168.35(10) . . ? C11 Fe1 C2 130.02(10) . . ? C14 Fe1 C4 171.00(11) . . ? C10 Fe1 C4 146.69(10) . . ? C12 Fe1 C4 108.62(9) . . ? C11 Fe1 C4 115.02(9) . . ? C2 Fe1 C4 68.51(8) . . ? C14 Fe1 C13 40.44(11) . . ? C10 Fe1 C13 67.97(10) . . ? C12 Fe1 C13 39.94(11) . . ? C11 Fe1 C13 67.32(10) . . ? C2 Fe1 C13 150.02(10) . . ? C4 Fe1 C13 131.58(10) . . ? C14 Fe1 C3 147.95(11) . . ? C10 Fe1 C3 114.60(10) . . ? C12 Fe1 C3 129.83(10) . . ? C11 Fe1 C3 107.16(9) . . ? C2 Fe1 C3 40.80(8) . . ? C4 Fe1 C3 40.72(8) . . ? C13 Fe1 C3 168.93(11) . . ? C14 Fe1 C1 110.30(9) . . ? C10 Fe1 C1 131.63(9) . . ? C12 Fe1 C1 149.94(10) . . ? C11 Fe1 C1 169.57(10) . . ? C2 Fe1 C1 40.73(8) . . ? C4 Fe1 C1 68.50(8) . . ? C13 Fe1 C1 118.47(10) . . ? C3 Fe1 C1 68.61(8) . . ? C14 Fe1 C5 132.93(10) . . ? C10 Fe1 C5 171.38(10) . . ? C12 Fe1 C5 117.30(9) . . ? C11 Fe1 C5 147.84(9) . . ? C2 Fe1 C5 68.40(8) . . ? C4 Fe1 C5 40.50(8) . . ? C13 Fe1 C5 110.79(9) . . ? C3 Fe1 C5 68.35(8) . . ? C1 Fe1 C5 40.74(8) . . ? C19 Fe2 C18 40.99(9) . . ? C19 Fe2 C25 122.56(9) . . ? C18 Fe2 C25 158.66(10) . . ? C19 Fe2 C24 107.06(9) . . ? C18 Fe2 C24 122.18(9) . . ? C25 Fe2 C24 40.88(9) . . ? C19 Fe2 C26 158.94(9) . . ? C18 Fe2 C26 158.91(10) . . ? C25 Fe2 C26 40.68(9) . . ? C24 Fe2 C26 68.49(9) . . ? C19 Fe2 C17 68.50(9) . . ? C18 Fe2 C17 40.58(9) . . ? C25 Fe2 C17 159.45(10) . . ? C24 Fe2 C17 158.29(9) . . ? C26 Fe2 C17 123.29(9) . . ? C19 Fe2 C27 158.60(9) . . ? C18 Fe2 C27 122.46(9) . . ? C25 Fe2 C27 68.45(9) . . ? C24 Fe2 C27 68.22(9) . . ? C26 Fe2 C27 40.74(9) . . ? C17 Fe2 C27 107.72(9) . . ? C19 Fe2 C16 68.48(9) . . ? C18 Fe2 C16 68.54(9) . . ? C25 Fe2 C16 123.24(9) . . ? C24 Fe2 C16 159.36(9) . . ? C26 Fe2 C16 108.01(9) . . ? C17 Fe2 C16 40.71(9) . . ? C27 Fe2 C16 123.30(9) . . ? C19 Fe2 C28 122.52(9) . . ? C18 Fe2 C28 107.03(9) . . ? C25 Fe2 C28 68.38(9) . . ? C24 Fe2 C28 40.45(9) . . ? C26 Fe2 C28 68.31(9) . . ? C17 Fe2 C28 122.68(9) . . ? C27 Fe2 C28 40.44(9) . . ? C16 Fe2 C28 158.98(9) . . ? C19 Fe2 C15 40.84(8) . . ? C18 Fe2 C15 68.91(8) . . ? C25 Fe2 C15 107.40(9) . . ? C24 Fe2 C15 122.79(9) . . ? C26 Fe2 C15 122.96(8) . . ? C17 Fe2 C15 68.64(9) . . ? C27 Fe2 C15 159.30(9) . . ? C16 Fe2 C15 40.74(8) . . ? C28 Fe2 C15 158.75(9) . . ? C31 Fe3 C32 40.81(9) . . ? C31 Fe3 C42 125.05(10) . . ? C32 Fe3 C42 105.99(9) . . ? C31 Fe3 C41 106.10(9) . . ? C32 Fe3 C41 117.08(9) . . ? C42 Fe3 C41 40.62(9) . . ? C31 Fe3 C38 163.46(10) . . ? C32 Fe3 C38 126.41(10) . . ? C42 Fe3 C38 40.83(10) . . ? C41 Fe3 C38 68.43(9) . . ? C31 Fe3 C33 68.51(9) . . ? C32 Fe3 C33 40.75(9) . . ? C42 Fe3 C33 118.52(9) . . ? C41 Fe3 C33 151.91(9) . . ? C38 Fe3 C33 108.51(9) . . ? C31 Fe3 C40 118.47(9) . . ? C32 Fe3 C40 151.86(9) . . ? C42 Fe3 C40 68.33(9) . . ? C41 Fe3 C40 40.61(9) . . ? C38 Fe3 C40 68.26(9) . . ? C33 Fe3 C40 166.39(9) . . ? C31 Fe3 C30 40.74(9) . . ? C32 Fe3 C30 68.56(9) . . ? C42 Fe3 C30 163.33(10) . . ? C41 Fe3 C30 126.48(9) . . ? C38 Fe3 C30 154.82(10) . . ? C33 Fe3 C30 68.35(9) . . ? C40 Fe3 C30 108.58(9) . . ? C31 Fe3 C39 153.57(9) . . ? C32 Fe3 C39 165.21(9) . . ? C42 Fe3 C39 68.42(9) . . ? C41 Fe3 C39 68.25(9) . . ? C38 Fe3 C39 40.61(9) . . ? C33 Fe3 C39 128.67(9) . . ? C40 Fe3 C39 40.44(9) . . ? C30 Fe3 C39 120.63(9) . . ? C31 Fe3 C29 68.71(9) . . ? C32 Fe3 C29 68.77(9) . . ? C42 Fe3 C29 153.72(9) . . ? C41 Fe3 C29 165.11(9) . . ? C38 Fe3 C29 120.41(9) . . ? C33 Fe3 C29 40.75(8) . . ? C40 Fe3 C29 128.42(9) . . ? C30 Fe3 C29 40.72(9) . . ? C39 Fe3 C29 109.79(9) . . ? C55 Fe4 C44 120.88(9) . . ? C55 Fe4 C45 106.44(9) . . ? C44 Fe4 C45 40.74(8) . . ? C55 Fe4 C54 40.73(9) . . ? C44 Fe4 C54 107.23(9) . . ? C45 Fe4 C54 123.35(9) . . ? C55 Fe4 C46 123.10(9) . . ? C44 Fe4 C46 68.53(8) . . ? C45 Fe4 C46 40.63(9) . . ? C54 Fe4 C46 159.76(9) . . ? C55 Fe4 C53 68.19(9) . . ? C44 Fe4 C53 124.49(9) . . ? C45 Fe4 C53 160.41(9) . . ? C54 Fe4 C53 40.43(9) . . ? C46 Fe4 C53 158.08(9) . . ? C55 Fe4 C56 40.64(9) . . ? C44 Fe4 C56 156.46(9) . . ? C45 Fe4 C56 120.99(9) . . ? C54 Fe4 C56 68.30(9) . . ? C46 Fe4 C56 107.23(8) . . ? C53 Fe4 C56 68.04(9) . . ? C55 Fe4 C43 157.05(8) . . ? C44 Fe4 C43 40.94(8) . . ? C45 Fe4 C43 68.77(8) . . ? C54 Fe4 C43 121.88(8) . . ? C46 Fe4 C43 68.75(8) . . ? C53 Fe4 C43 108.40(8) . . ? C56 Fe4 C43 161.13(9) . . ? C55 Fe4 C47 160.32(8) . . ? C44 Fe4 C47 68.40(8) . . ? C45 Fe4 C47 68.36(9) . . ? C54 Fe4 C47 157.95(9) . . ? C46 Fe4 C47 40.73(8) . . ? C53 Fe4 C47 122.97(9) . . ? C56 Fe4 C47 124.43(8) . . ? C43 Fe4 C47 40.68(8) . . ? C55 Fe4 C52 68.28(9) . . ? C44 Fe4 C52 161.45(9) . . ? C45 Fe4 C52 156.85(9) . . ? C54 Fe4 C52 68.27(9) . . ? C46 Fe4 C52 121.99(9) . . ? C53 Fe4 C52 40.57(9) . . ? C56 Fe4 C52 40.40(9) . . ? C43 Fe4 C52 124.89(9) . . ? C47 Fe4 C52 108.60(9) . . ? C8 N1 C9 110.27(17) . . ? C8 N1 C7 110.86(16) . . ? C9 N1 C7 112.86(16) . . ? C22 N2 C23 110.2(2) . . ? C22 N2 C21 112.14(19) . . ? C23 N2 C21 111.80(18) . . ? C37 N3 C36 110.32(18) . . ? C37 N3 C35 113.31(19) . . ? C36 N3 C35 110.39(17) . . ? C51 N4 C50 110.27(18) . . ? C51 N4 C49 112.51(17) . . ? C50 N4 C49 111.61(16) . . ? C2 C1 C5 107.47(18) . . ? C2 C1 C6 125.49(18) . . ? C5 C1 C6 126.95(19) . . ? C2 C1 Fe1 69.16(11) . . ? C5 C1 Fe1 69.64(11) . . ? C6 C1 Fe1 129.11(14) . . ? C3 C2 C1 108.36(18) . . ? C3 C2 Fe1 69.77(11) . . ? C1 C2 Fe1 70.11(11) . . ? C4 C3 C2 107.69(19) . . ? C4 C3 Fe1 69.53(11) . . ? C2 C3 Fe1 69.43(11) . . ? C5 C4 C3 108.35(18) . . ? C5 C4 Fe1 70.18(11) . . ? C3 C4 Fe1 69.75(11) . . ? C4 C5 C1 108.12(18) . . ? C4 C5 Fe1 69.33(12) . . ? C1 C5 Fe1 69.62(11) . . ? C1 C6 C7 111.77(17) . . ? N1 C7 C6 112.58(16) . . ? C11 C10 C14 107.4(2) . . ? C11 C10 Fe1 69.88(13) . . ? C14 C10 Fe1 69.62(13) . . ? C12 C11 C10 108.4(2) . . ? C12 C11 Fe1 70.00(14) . . ? C10 C11 Fe1 69.75(13) . . ? C11 C12 C13 108.7(2) . . ? C11 C12 Fe1 70.09(14) . . ? C13 C12 Fe1 70.23(14) . . ? C12 C13 C14 108.0(2) . . ? C12 C13 Fe1 69.83(13) . . ? C14 C13 Fe1 69.52(13) . . ? C13 C14 C10 107.6(2) . . ? C13 C14 Fe1 70.04(13) . . ? C10 C14 Fe1 69.69(13) . . ? C16 C15 C19 107.22(19) . . ? C16 C15 C20 124.65(19) . . ? C19 C15 C20 128.1(2) . . ? C16 C15 Fe2 69.32(11) . . ? C19 C15 Fe2 69.01(11) . . ? C20 C15 Fe2 128.43(15) . . ? C17 C16 C15 108.36(19) . . ? C17 C16 Fe2 69.61(12) . . ? C15 C16 Fe2 69.94(12) . . ? C18 C17 C16 108.2(2) . . ? C18 C17 Fe2 69.50(13) . . ? C16 C17 Fe2 69.68(12) . . ? C17 C18 C19 107.8(2) . . ? C17 C18 Fe2 69.92(12) . . ? C19 C18 Fe2 69.48(12) . . ? C15 C19 C18 108.4(2) . . ? C15 C19 Fe2 70.15(11) . . ? C18 C19 Fe2 69.53(12) . . ? C15 C20 C21 113.80(17) . . ? N2 C21 C20 111.61(17) . . ? C28 C24 C25 107.9(2) . . ? C28 C24 Fe2 69.88(12) . . ? C25 C24 Fe2 69.48(12) . . ? C26 C25 C24 107.8(2) . . ? C26 C25 Fe2 69.75(12) . . ? C24 C25 Fe2 69.64(13) . . ? C25 C26 C27 107.84(19) . . ? C25 C26 Fe2 69.57(12) . . ? C27 C26 Fe2 69.63(12) . . ? C28 C27 C26 108.1(2) . . ? C28 C27 Fe2 69.87(12) . . ? C26 C27 Fe2 69.63(12) . . ? C27 C28 C24 108.3(2) . . ? C27 C28 Fe2 69.69(12) . . ? C24 C28 Fe2 69.67(12) . . ? C30 C29 C33 107.2(2) . . ? C30 C29 C34 125.88(19) . . ? C33 C29 C34 126.74(19) . . ? C30 C29 Fe3 69.28(12) . . ? C33 C29 Fe3 69.23(12) . . ? C34 C29 Fe3 130.21(15) . . ? C31 C30 C29 108.41(19) . . ? C31 C30 Fe3 69.38(12) . . ? C29 C30 Fe3 70.00(12) . . ? C30 C31 C32 108.0(2) . . ? C30 C31 Fe3 69.88(12) . . ? C32 C31 Fe3 69.61(12) . . ? C31 C32 C33 107.85(19) . . ? C31 C32 Fe3 69.58(12) . . ? C33 C32 Fe3 69.82(12) . . ? C32 C33 C29 108.50(19) . . ? C32 C33 Fe3 69.43(12) . . ? C29 C33 Fe3 70.03(11) . . ? C29 C34 C35 112.24(17) . . ? N3 C35 C34 113.46(17) . . ? C39 C38 C42 108.0(2) . . ? C39 C38 Fe3 70.14(12) . . ? C42 C38 Fe3 69.52(13) . . ? C40 C39 C38 107.8(2) . . ? C40 C39 Fe3 69.45(12) . . ? C38 C39 Fe3 69.25(12) . . ? C39 C40 C41 108.28(19) . . ? C39 C40 Fe3 70.11(12) . . ? C41 C40 Fe3 69.55(12) . . ? C42 C41 C40 108.1(2) . . ? C42 C41 Fe3 69.65(12) . . ? C40 C41 Fe3 69.84(12) . . ? C41 C42 C38 107.9(2) . . ? C41 C42 Fe3 69.73(12) . . ? C38 C42 Fe3 69.65(13) . . ? C47 C43 C44 107.31(18) . . ? C47 C43 C48 128.08(19) . . ? C44 C43 C48 124.54(18) . . ? C47 C43 Fe4 69.68(11) . . ? C44 C43 Fe4 69.25(11) . . ? C48 C43 Fe4 128.42(14) . . ? C45 C44 C43 108.21(18) . . ? C45 C44 Fe4 69.63(11) . . ? C43 C44 Fe4 69.82(11) . . ? C46 C45 C44 108.19(19) . . ? C46 C45 Fe4 69.78(12) . . ? C44 C45 Fe4 69.63(12) . . ? C45 C46 C47 107.87(18) . . ? C45 C46 Fe4 69.58(12) . . ? C47 C46 Fe4 69.83(11) . . ? C43 C47 C46 108.41(19) . . ? C43 C47 Fe4 69.65(11) . . ? C46 C47 Fe4 69.43(11) . . ? C43 C48 C49 112.89(16) . . ? N4 C49 C48 111.83(16) . . ? C56 C52 C53 107.6(2) . . ? C56 C52 Fe4 69.57(12) . . ? C53 C52 Fe4 69.43(12) . . ? C54 C53 C52 108.41(19) . . ? C54 C53 Fe4 69.67(12) . . ? C52 C53 Fe4 70.01(12) . . ? C53 C54 C55 107.89(19) . . ? C53 C54 Fe4 69.90(12) . . ? C55 C54 Fe4 69.59(12) . . ? C56 C55 C54 107.8(2) . . ? C56 C55 Fe4 69.91(12) . . ? C54 C55 Fe4 69.68(12) . . ? C52 C56 C55 108.24(19) . . ? C52 C56 Fe4 70.02(12) . . ? C55 C56 Fe4 69.45(12) . . ? F2B B1 F4A 139.5(4) . . ? F2B B1 F1B 116.2(7) . . ? F4A B1 F1B 102.9(6) . . ? F2B B1 F3A 37.0(3) . . ? F4A B1 F3A 116.4(4) . . ? F1B B1 F3A 134.9(6) . . ? F2B B1 F2A 105.4(6) . . ? F4A B1 F2A 114.8(6) . . ? F1B B1 F2A 24.7(7) . . ? F3A B1 F2A 112.4(5) . . ? F2B B1 F4B 112.0(4) . . ? F4A B1 F4B 36.9(2) . . ? F1B B1 F4B 113.4(5) . . ? F3A B1 F4B 111.3(3) . . ? F2A B1 F4B 136.0(5) . . ? F2B B1 F3B 105.6(3) . . ? F4A B1 F3B 70.8(3) . . ? F1B B1 F3B 106.5(6) . . ? F3A B1 F3B 69.6(4) . . ? F2A B1 F3B 89.5(5) . . ? F4B B1 F3B 101.6(3) . . ? F2B B1 F1A 69.3(3) . . ? F4A B1 F1A 104.5(3) . . ? F1B B1 F1A 86.8(6) . . ? F3A B1 F1A 102.9(4) . . ? F2A B1 F1A 103.8(6) . . ? F4B B1 F1A 70.2(3) . . ? F3B B1 F1A 166.5(3) . . ? F8A B2 F7A 115.6(5) . . ? F8A B2 F5B 143.3(5) . . ? F7A B2 F5B 96.3(3) . . ? F8A B2 F7B 82.4(4) . . ? F7A B2 F7B 46.7(3) . . ? F5B B2 F7B 110.5(2) . . ? F8A B2 F8B 35.2(4) . . ? F7A B2 F8B 150.2(4) . . ? F5B B2 F8B 110.0(3) . . ? F7B B2 F8B 108.7(3) . . ? F8A B2 F6B 95.7(4) . . ? F7A B2 F6B 74.0(4) . . ? F5B B2 F6B 110.8(2) . . ? F7B B2 F6B 109.1(2) . . ? F8B B2 F6B 107.5(2) . . ? F8A B2 F5A 115.1(7) . . ? F7A B2 F5A 104.9(5) . . ? F5B B2 F5A 34.1(4) . . ? F7B B2 F5A 92.3(4) . . ? F8B B2 F5A 90.6(5) . . ? F6B B2 F5A 144.9(5) . . ? F8A B2 F6A 106.4(4) . . ? F7A B2 F6A 112.2(5) . . ? F5B B2 F6A 74.9(3) . . ? F7B B2 F6A 157.7(4) . . ? F8B B2 F6A 88.4(3) . . ? F6B B2 F6A 50.5(3) . . ? F5A B2 F6A 101.9(6) . . ? F9 B3 F12 110.0(2) . . ? F9 B3 F10 109.9(2) . . ? F12 B3 F10 110.0(2) . . ? F9 B3 F11 110.9(2) . . ? F12 B3 F11 108.7(2) . . ? F10 B3 F11 107.22(19) . . ? F13A B4 F15A 97.2(7) . . ? F13A B4 F16B 119.6(6) . . ? F15A B4 F16B 127.8(5) . . ? F13A B4 F14A 124.9(5) . . ? F15A B4 F14A 120.3(6) . . ? F16B B4 F14A 68.7(4) . . ? F13A B4 F16A 91.2(6) . . ? F15A B4 F16A 110.1(4) . . ? F16B B4 F16A 41.0(4) . . ? F14A B4 F16A 109.3(4) . . ? F13A B4 F14B 112.8(6) . . ? F15A B4 F14B 87.7(5) . . ? F16B B4 F14B 107.6(5) . . ? F14A B4 F14B 40.4(3) . . ? F16A B4 F14B 148.5(4) . . ? F13A B4 F13B 21.0(7) . . ? F15A B4 F13B 108.8(6) . . ? F16B B4 F13B 118.7(5) . . ? F14A B4 F13B 104.1(5) . . ? F16A B4 F13B 102.8(5) . . ? F14B B4 F13B 95.1(5) . . ? F13A B4 F15B 112.1(6) . . ? F15A B4 F15B 21.7(5) . . ? F16B B4 F15B 106.1(5) . . ? F14A B4 F15B 116.9(5) . . ? F16A B4 F15B 93.3(4) . . ? F14B B4 F15B 95.9(4) . . ? F13B B4 F15B 127.7(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.361 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.089